Glucose treatment of feathers



United States Patent "ice Ohio, assignors to the United States of America as represented by the Secretary of the Army No Drawing. Application May 17, 1957 Serial No. 660,015

11 Claims. ((31. 8-94.10

This invention relates to a method of-treating land fowl feathers, especially chicken feathers, to increase their filling power and resiliency, and to impart 'permanent curliness and water repellency, thereby making such feathers an acceptable substitute for the standard down and feather mixture now in wide use for sleeping bags, comforts, etc. Another object is to provide a treatment which enables the feathers to retain much of their high filling power after several washings with a detergent. A further object is to make feathers resistant to microbiological attack. Other objects will be apparent from the following description of the method presently preferred by us.

In explanation of the term filling power, reference may be made to the report entitled A Proposed Method for Measuring the Filling Power of Down and Feathers, by'Henry A. Sinski, publication No. TD 103037, The Otfice of Technical Services, Department of Commerce, and to the article by N. B. Edelman in Textile Research Journal, vol. 17, page 199 (April 1947) entitled Investigation of Methods for Determining the Filling Power of Feathers, See also the Sinski et al. Patent No. 2,706,- 910, dated April 26, 1955. Ordinarily, chicken feathers have a filling power of 1.8 to 2.1 cm., while the 40/60 down-feather mixture has a filling power of 5.3 to

The term feathers as used herein includes whole land fowl feathers of the desired size range, crushed (commercial curled) land fowl feathers, land fowl feather fibers, stripped land fowl feathers, and mixtures of these.

In the preferred procedure, the feathers, if not known to be entirely free from blood, are first soaked for about ten minutes in a water solution of a commercial blood solubilizer, such as Haemo-Sol or Coagusol. After the soaking, the solution is drained from the feathers and the feathers are then laundered or dry cleaned. In laundering, preferably a detergent such as Tergitol NPX is used (0.25% water solution at 110l25 F.). Other detergents which have been found to be satisfactory are sold under the trade names or trademarks Sted, Glim, Triton, Sterox and Monsanto MXP. In general, the non-ionic type of detergents should be used to obviate any action on the protein of the feathers. Laundering continues for about twenty minutes, then the solution is removed from the feathers by centrifuging or wringing. While a number of well-known dry cleaning solutions could be used to clean the feathers, laundering is preferred because it is less expensive. Both laundering and dry cleaning may take place in the same vessel or container that is used during the blood-solubilizing step. Of course, if the feathers as initially received are perfectly clean, the soaking and washing or dry cleaning may be omitted.

If the feathers are from immature chickens, the damp feathers from the described laundering or dry cleaning operation are placed in a 1% water solution of trisodium 2,886,400 Patented May 12, 1959 phosphate Na -P0 .12H O at '43-'-44 C. for about ten minutes. If feathers from mature chickens are being processed, the phosphate treatment period is increased to about thirty minutes. This mild alkaline treatment of the feathers is believed to alter the stability of the feathers by modification of the cystine linkages in the keratin. This step is important because it materially increases the curliness of the feathers and it curls naturally unciirly mature feathers, thereby to increase the bulk value of the final feather product. Other suitably buffered alkaline solutions, for example, sodium carbonate or bor'ax, may be used in lieu of the phosphate solution mentioned above, but in all cases the time of the treatment must be less for immature feathers to avoid excessive degradation. Trisodium phosphate is preferred because of its quicker action due to a higher pH. It is believed that the higher concentration of cystine linkages in mature feathers enables them to resist the action of the alkaline-solution for a longer period.

The data from several successful laboratory runs at The Tanners Council Research Laboratory, University of Cincinnati, will now be given.

Glucose chromic acid-hydrazine treatment A 67 gram batch of chicken feathers was first soaked in the phosphate solution mentioned above for thirty minutes with occasional agitation. Then the feathers were rinsed to neutrality and were immersed in a bath consisting of 3 liters of 3.2% glucose solution (H O) in the presence of a catalyst, preferably 6 grams of aluminum sulfate A1 SO .18H O and dilute sulfuric acid, at pH 2.7-2.8 and 43-45 C. Or the bath may be a 1.6% glucose solution containing 0.1% aluminum sul- "fate anddilute sulfuric acid, at the same pH and tempera'ture range.

The feathers remained in this bath for thirty minutes, then the pH of the glucose solution was raised gradually with 15% Na CO solution to pH 7.1 and the'feathers were kept in the neutral bath for fifteen minutes more at 42 C. In lieu of aluminum sulfate, other salts such as chromium sulfate or zirconium sulfate could be used but aluminum sulfate is preferred. Then the feathers were removed from the bath and washed to remove the unreacted glucose from the feathers. Next the feathers were placed in a chromic acid bath (30 g. Na Cr O- .2H O in 3000 ml. of water plus 4 ml. of concentrated sulfuric acid) and kept there for two hours at pH 2.5-2.7 and a temperature of 39- 43 C. After this the spent chrome liquor was drained off and the feathers were transferred to a reducing bath prepared from 12 grams of hydrazine sulfate and 2500 ml. of water and 500 ml. of spent chromic acid solution. After 30 to 60 minutes in this reducing bath at pH 4.2 and a temperature of 3843 C., the pH was raised to 7.0 by adding dilute sodium carbonate solution, and the feathers were kept in this nearly neutral bath for ten minutes longer. Then the feathers were removed, rinsed for twenty minutes, dried and relaxed. The filling power was 6.4 cm.

All the feathers treated as above were additionally treated with 1500 ml. of a silicone resin solution of 9.2% strength in an inert organic solvent, such as Stoddard solvent (a refined petroleum hydrocarbon solvent) at 25 30 C. for one hour with occasional stirring. The feathers were removed, dried and relaxed. The filling power was then 8.3 cm. After laundering, the filling power was almost exactly the same. Evidently, the silicone resin adhered to the treated feathers to give them a coating that resists water and detergents.

Glucose-"Tanolin R treatment A 67 gram batch of chicken feathers was given the phosphate treatment described above, then was well rinsed with water. J The feathers were then put in a bath of 3 liters of 3.2% glucose dissolved in water, containing 6 grams of Tanolin R and 50 ml. of dilute sulfuric acid. Tanolin R is a trade name for one-third basic chromic sulfate" containing about chromicoxide.. The feathersrernained in this bath 'forthirtyminutes at .pH 2.7, thestemperatureubeing .about 44-?.'C. Then the pH was 'raisedto 7.1;.and;.the feathers. were kept .in the :neutral 'solutiontat :4244. .C. .for .fifteen minutes longer. The feathers: were thenremoved, :rinsed forltwenty-five. minutes, :then 1 driedand relaxed; The filling power was 6.3. 'In lieu of .TanolinR, which is a catalyst, aluminum sulfate,.chromium sulfate or zirconium sulfate can .be .used with substantiallythe same results, gi

A -gran1. batch of. theabove-treatedieathers was fruther subjected to a" surface treatmentlby immersion in a 9.4%. solutionof silicone resin in .1000ml. of Stoddard solvent. Iheperiodof the treatment maybe one to two:hours at. about 24 C., with occasional stirring. Then the feathers were removed, centrifuged, then tumble-dried atiroomitemperaturef.The filling. power was 9.6 cm. After launderingand drying .in channels (to simulate the conditions feathers are. subjected. to when in sleepingbags), the fillingpower was 8.6 cm.. But on removing the feathers. and allowing them to relax for several. weeks, the filling power rose to 9.2 cm. 7 In many other trials, high 'filling power has been imparted to chicken feathers byjreatment with glucose solution, oxidation with chromic acid, and reduction with hydrazine; Invariablyjthefilling :power readings improved'upon aging, *whether} or not the: feathers were laundered after treatment, The feathers of this process showcomplete resistance to papain-bisulfite attack, which We consider to be jofmajor importance. 7 "i l y -What we claimis: ff

' 1. A method of treating fowl feathers to enhance their filling power which comprises placing the feathers in a' bath'of a glucose solution of about 1.6"3. 2% strength in the presence of a catalytic amountof a metallic salt catalyst at pH ,about'2,7-2 .8 for about half an hour and at about 43 45 C., said catalyst'being'a member of the group consistingof aluminum sulfate, chromium sulfate, and zirconium sulfateg' then raising the pH to abou t neutral and keeping the feathers in thebath until mid feathers. are'substantially neutralized; then removing the feafliers from the bath and washing them to remove the ,unreacted. glucose;v then placing .the feathers in. a .dilute chromic acid bath at pH about 2.5-2.7 and a temperature of about 39-43 C.; then substantially neutralizing the bath and allowing the feathers to remain therein for at least about ten minutes; then removing the feathers, from said bath, and rinsing and ,drying them.

2. Theinventiondefined in claim 1, wherein the feathers are given a curling treatment, priorto the glucose treatment, by means of a warm aqueous alkalinephosphate solution, thefeathers beingrinsed after the alkaline phosphate bath.

3. The invention defined in claim 2, wherein the curling treatment is imparte'd by an about 6% to 1% water solution of trisodium phosphate at about 4344 C for about ten minutesto thirty minutes} 4. A method of treating land fowl feathers according to claim 1, wherein said feathers are transferred from lsaid chromic acid bath to .a reducing -bath,. said reducing 'bathbeing a dilute hydrazine solutions 5.: The invention defined in claim 4, wherein the land fowl ifeathers are first soaked in an: about 0.5-to 1 percent solution of sodium phosphatefor about thirty minutes at about 4331-1-44" C. to induce a curl,-th'en are rinsed before undergoing the glucosetreatment.

. 6. .Theinvention defined in claim 4, wherein the catalyst is aluminum sulfate plus dilute sulfuric acid and the chromic acid bathis :an 'about..1% sodium bichromate solution containing about 0.25 sulfuric acid.

- .7. The invention .define'd in claim 4, wherein the treated and substantially dry land fowl feathers are finally; given asurface treatment ,by immersing them in. .a silicone resin i dissolved in an inert organic. solvent.

'8.:;Th'e product. produced-by the method oflclaim 1. 9.,The product produced by the method ofclaim 3. 10. The product produced by the method of claim 4. '11.,The' product produced by the method of claim 7. 

1. A METHOD OF TREATING LAND FOWL FEATHERS TO ENHANCE THEIR FILLING POWER WHICH COMPRISES PLACING THE FEATHERS IN A BATH OF A GLUCOSE SOLUTION OF ABOUT 1.6-3.2% STRENGTH IN THE PRESENCE OF A CATALYTIC AMOUNT OF A METALLIC SALT CATALYST AT PH ABOUT 297-2.8 FOR ABOUT HALF AN HOUR AND AT ABOUT 43*-45*C., SAID CATALYST BEING A MEMBER OF THE GROUP CONSISTING OF ALUMINUM SULFATE, CHROMIUM SULFATE, AND ZIRCONIUM SULFATE; THEN RAISING THE PH TO ABOUT NUETRAL AND KEEPING THE FEATHERS IN THE BATH UNTIL SAID FEATHERS ARE SUBSTANTIALLY NEUTRALIZED; THEN REMOVING THE FEATHERS FROM THE BATH AND WASHING THEM TO REMOVE THE UNREACTED GLUCOSE; THEN PLACING THE FEATHERS IN A DILUTE CHROMIC ACID BATH AT PH ABOUT 2.5-2.7 AND A TEMPERATURE OF ABOUT 39*-43*C., THEN SUBSTANTIALLY NEUTRALIZING THE BATH AND ALLOWING THE FEATHERS TO REMAIN THEREIN FOR AT LEAST ABOUT TEN MINUTED; THEN REMOVING THE FEATHERS, FROM SAID BATH, AND RINSING SAID DRYING THEM. 